CAJ | 학술논문

芳纶纤维在合成过程中常使用N-甲基吡咯烷酮作为反应溶剂，通过对提取方法和色谱、质谱条件的改进，建立了芳纶纤维中溶剂残留物N-甲基吡咯烷酮(NMP)的气相色谱-质谱联用(GC/MS)测定法.芳纶纤维试样经乙酸乙酯超声波提取，提取液浓缩后用滤纸过滤，用气相色谱-质谱仪测定，外标法定量，选择离子监测进行阳性确证.结果表明，当添加N-甲基吡咯烷酮1~10μg/mL时，待测芳纶纤维试样中N-甲基吡咯烷酮的回收率达95.8%，相对标准偏差RSD(n=7)小于5％，其最低检出限为0.05μg/mL.本方法操作简单、灵敏度高、重现性好，可用于芳纶纤维中N-甲基吡咯烷酮残留量分析.
방륜섬유재합성과정중상사용N-갑기필각완동작위반응용제，통과대제취방법화색보、질보조건적개진，건립료방륜섬유중용제잔류물N-갑기필각완동(NMP)적기상색보-질보련용(GC/MS)측정법.방륜섬유시양경을산을지초성파제취，제취액농축후용려지과려，용기상색보-질보의측정，외표법정량，선택리자감측진행양성학증.결과표명，당첨가N-갑기필각완동1~10μg/mL시，대측방륜섬유시양중N-갑기필각완동적회수솔체95.8%，상대표준편차RSD(n=7)소우5％，기최저검출한위0.05μg/mL.본방법조작간단、령민도고、중현성호，가용우방륜섬유중N-갑기필각완동잔류량분석.
N-methylpyrrolidinone (NMP) was commonly used as reaction solvents in the synthesis of ara-mid fiber. A gas chromatography/mass spectrometry (GC/MS) method of determination of N-methylpyrrolidi-none in textiles was established by improving the extraction method and GC/MS conditions. The samples were extracted with ethyl acetate by ultrasound assisted procedure.After being concentrated and purified with filter paper, the extract was quantitatively determined using GC/MS by external standard method and positive-ly confirmed through selected-ion monitoring mode. The results showed that while the dosage of N-methyl-pyrrolidinone was 1~10 μg/mL, the method provided 95.8% of recovery rate, lower than 5% of relative stan-dard deviations and 0.05 μg/mL of determination limit. The method was simple, and had high sensitivity and good repeatability, which could be used in the residual content determination of NMP in aramid fiber.